Method of treating rosin and rosin product



Patented Aug. 11, 1936 UNITED STATES PATENT OFFICE,

METHOD OF TREATING ROSIN AND ROSIN PRODUCT ration of Delaware NoDrawing. Original application November 19,

1931, Serial No. 576,200. Divided and this application April 5, 1934,Serial No. 719,146

14 Claims.

This invention relates to a method of treating rosin, as wood or gumrosin, and to a novel and advantageous rosin product.

More particularly, this invention relates to a method of treating rosinby which a novel and advantageous rosin product may be obtained and bywhich, at the same time, a refined or purified rosin is obtained. Thenovel rosin product will be found to be insoluble in gasoline, solublein alcohol, it may be decomposed by water and will be found to beadvantageously adaptable for various use in the commercial arts. Therefined or purified rosin produced will be found to be purified orrefined more particularly by the elimination of coloring matter or colorbodies and hence where a low grade rosin is subjected to treatment inaccordance with the method of this invention, a rosin of high colorgrade may be obtained.

In accordance with the method embodying this invention, rosin, as woodor gum rosin, is subjected to treatment with an alkylamine, as forexample, mono-, di-, and polyalkylamines, the alkylamine preferablybeing an hydroxy alkylamine. The rosin is preferably treated in solutionin a suitable solvent therefor. As a result of the treatment thealkylamine will react with the rosin for the formation of a precipitatecomprising largely the reaction product of oxidized abietic acid, colorbodies and other reactive constituents of the rosin with the alkylamine.The precipitate will also contain more or less reaction product of thereaction of abietic acid with the alkylamine, depending upon the amountof alkylamine used in the treatment. The novel product in accordancewith this invention will comprise the precipitate described, while therosin remaining in the treated solution may be recovered as refined orpurified rosin after separation from the precipitate. It will beappreciated that by control within wide limits of the amount ofalkylamine used for the treatment of any given amount of rosin, therelative proportions of novel product or of refined rosin may be varied.

In proceeding in accordance with the method embodying this invention, ashas been indicated, the rosin, which may be either wood or gum rosin,may be subjected to treatment in solution in a suitable solvent forrosin, as gasoline or other light petroleum distillate. The function ofthe solvent is primarily to effect dispersion of the rosin to enableefficient contact between the rosin and the alkylamine and the solventdoes not enter into the reaction involved. Hence, it may be any suitablesolvent for rosin which is non-aqueous and non-reactive with thealkylamine used for the treatment.

The alkylamine, as has been indicated, may be a mono-, di-, orpolyalkylamine and may be an ethanolamine, a methanolamine, or the like.For example, we may use mono-, di-, or tri-ethanolamine or similarmethanolamines, glycerolamine, etc., and preferably such containing ahydroxy group. It will be appreciated that the alkylamines may be usedin admixture and that, for example, various of the polyalkylamines willcontain some mono-, and/or diamines, especially where the commercialgrade is'used. Thus, for example, commercial triethanolamine, while itcontains a preponderating proportion of triethanolamine, will alsocontain considerable quantities of monoand diethanolamine.

In carrying out the method embodying this invention, by way ofillustration, for example, 300 parts of a 15% solution in gasoline ofwood rosin, grading, for example, FF in color, are washed by agitationwith, for example, 3 parts of triethanolamine. The precipitate formed isseparated from the gasoline-rosin solution by drawing off the solutionor by filtration. The separated gasolinerosin solution is desirablywashed with Water and the gasoline then evaporated. The rosin recoveredfrom the gasoline-rosin solution will amount to about 89% of the rosintreated and will be found to be purified and refined and to grade H incolor.

The precipitate will comprise largely triethanolamine oxy-abietate andcolor bodies from the rosin treated. The trlethanolamine abietate willbe found to be insoluable in gasoline, soluble in alcohol and to havevarious uses in the commercial arts. The precipitate, as has beenindicated, may be decomposed by water and hence, if desired, may behydrolyzed, for example, with hot water to abietic acid, oxyabietic acidand triethanolamine. The abietic acid may then be recovered from thesolution by extraction with a solvent therefor, as for example,gasoline, or other light petroleum distillate, etc., and from theextract after its separation from the solutions a dark rosin, grading incolor somewhat darker than D, may be recovered by, for example,evaporation off of the solvent; and the triethanolamine may be recoveredfor reuse by evaporation off of the Water after separation from thegasoline-rosin extract. Desirably the solution may be filtered afterseparation of the gasoline extract and before evaporation of the waterfor recovery of the alkylamine.

As a further illustration, for example, 300 parts of a 15% solution ofrosin, grading, for example, FF in color, in gasoline are washed with 6parts of diethanolamine, the gasoline-rosin solution separated from theprecipitate formed and the gasoline recovered from the gasoline-rosinsolution by, for example, evaporating on the gasoline. .A 68% yield ofrosin grading H in color will be obtained from the gasoline-rosinsolution. The precipitate may be utilized as recovered or, if it bedesirable to recover the rosin therefrom and purifying agent therefrom,such may be efiected as indicated above after hydrolysis with water.

In carrying out the method in accordance with this invention, theprocedure may be carried out without the necessity for any particularform or type of apparatus and, as will be obvious, may be carried out asa'batch orcontinuous method. The treatment may be effected at roomtemperature or below, or if desired the temperature may be increased,avoiding, of course, the use of a temperature at which the solvent forthe rosin will be lost to any substantial extent during the treatment.

It will be appreciated, and as appears .from the above illustrations,that the alkylamine may be used in widely varying amounts, dependingupon the relative proportions of refined rosin precipitate, or newproduct, desired to be obtained. Where refined rosin is principallydesired, the maximum amount of alkylamine used will be limited by thedegree of purity or refinement desired for the rosin product. On'theother hand, where the precipitate, or new product, is primarily desired,the alkylamine may be used in quantity sutficient to react withsubstantially all of the rosin, or may be used in excess.

It will be understood that the terms oxyabietic acid and oxy-abietate asused herein and in the claims appended hereto are intended to includehydroxy-abietic acid and hydroxyabietate.

This application is a division of an application, Serial No. 576,200,filed November 19, 1931, by Joseph N. Borglin and Leavitt N. Bent, nowPatent No, 1,995,600, dated March 26, 1935.

What we claim and desire to protect by Letters Patent is:

1. As a new composition of matter an alkylamine oXy-abietate,

2. As a new composition of matter a polyalkylamine oxy-abietate.

3. As a new composition of matter an ethanolamine oxy-abietate.

4. As a new composition of matter a polyethanolamine oxy-abietate.

5. As a new composition of matter triethanolamine hydroXy-abietate.

6. As a new composition of matter triethanolamine oxy-abietate.

7. As a new composition of matter a glycerolamine oxy-abietate.

8. As a new composition of matter a polyglycerolamine oxy-abietate.

9. As a new composition of matter a triglycerolamine oxy-abietate.

l0. As a new composition of matter a methanolamine oxy-abietate.

11. As a new composition of matter a trimethanolamine oXy-abietate.

12. An alkylamine salt of oxidized abietic acid.

A polyalkylamine salt of oxidized abietic aci 14. An alkylamine salt ofhydroxy-abietic acid.

JOSEPH N. BORGLIN. LEAVITT N. BENT.

